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Method for refining carglumic acid

A technology of carboglutamate and carboglutamate, which is applied in chemical instruments and methods, preparation of urea derivatives, preparation of organic compounds, etc., can solve the problem of low purity and achieve the effect of extensive sources

Active Publication Date: 2018-05-11
WUHAN WUYAO SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the present invention mainly improves the post-purification process of carboglutamic acid, solves the problem of low purity of traditional craft products, especially reduces the maximum simple impurity content to a level below 0.1%, so that the quality of raw materials can be further declared Related Drug Products

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  • Method for refining carglumic acid
  • Method for refining carglumic acid
  • Method for refining carglumic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0042] 1.47kg of crude carglutamic acid and 5L of ethanol were mixed in a 10L three-neck flask, stirred and heated to 35°C, and a solution prepared by 800g of sodium hydroxide and 3200g of purified water was added thereto. After the addition, stir to clarify the reaction solution. Then keep stirring at 35°C for 0.5h, then cool to 15°C, and crystallize for 10h. Suction filtration to dryness, and drying to obtain 700 g of sodium salt of carboglutamic acid. Mix the above-mentioned ammonium salt with 6L of purified water into a 10L three-neck flask, stir to dissolve, then adjust the pH to 1-2 with acid, cool to 0°C, and crystallize for 10h. After the crystallization is completed, filter to dryness with suction and dry at 30° C. to obtain 370 g of refined glutamic acid, the product has a purity of 99.8%, and the maximum single impurity is less than 0.1%; the product yield is 25.2%.

Embodiment 2

[0044] Mix 4.8kg of crude carboglutamic acid and 20.4L of ethanol in a 50L reactor, stir and raise the temperature to 45°C, and add 13.7kg of concentrated ammonia water dropwise thereto. After the addition, continue to add 1.1kg of purified water, and the reaction solution is clarified. Then keep stirring at 45°C for 0.5h, then cool to 25°C, and crystallize for 20h. Suction filtration to dryness, and drying to obtain 2.3 kg of carboglutamic acid ammonium salt. Mix the above-mentioned ammonium salt with 19L of purified water into a 50L reactor, stir to dissolve, then adjust the pH to 1-2 with acid, cool to 10°C, and crystallize for 20h. After the crystallization is completed, the product is dried by centrifugation and dried at 30° C. to obtain 1.4 kg of refined glutamic acid, with a product content of 99.7 percent and a maximum simple impurity of less than 0.1 percent; the product yield is 29.2 percent.

Embodiment 3

[0046]Mix 4.8 kg of crude carboglutamic acid and 20.4 L of ethanol in a 50 L reactor, stir and heat up to 30° C., and dropwise add 13.7 kg of concentrated ammonia water therein. After the addition, continue to add 1.1kg of purified water, and the reaction solution is clarified. Then keep stirring at 30°C for 1h, then cool to 5°C, and crystallize for 10h. Suction filtration to dryness, and drying to obtain 2.3 kg of carboglutamic acid ammonium salt. Mix the above-mentioned ammonium salt with 19L of purified water into a 50L reactor, stir to dissolve, then adjust the pH to 1-2 with acid, cool to 0°C, and crystallize for 20 hours. After the crystallization is completed, the product is dried by centrifugation and dried at 30° C. to obtain 1.24 kg of refined glutamic acid, the product content is 99.8%, and the maximum simplex is less than 0.1%; the product yield is 25.8%.

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Abstract

The invention relates to a method for refining carglumic acid. The method comprises the following steps: (1-1) reacting crude carglumic acid with an alkali in a C1-5 alcohol solvent to obtain carglutamate; and (2-1) reacting the carglutamate obtained in step (1-1) with an acid to obtain the carglumic acid. The method solves the problem of low product purity of traditional technologies, and improves the product quality of the carglumic acid; and the content of the product refined through the method reaches 99.5% or more, the impurity content is less than 0.1%, and the product quality of a bulkdrug is met.

Description

technical field [0001] The invention relates to a method for refining carboglutamic acid, in particular to a method for reproducing carboglutamic acid by reacting a crude product with an alkali and further reacting with an acid. Background technique [0002] According to reports, between 1980 and 2001, 42 children from 28 families were diagnosed with NAGS (N-acetylglutamate synthetase) deficiency, and 8 of them died because they were not treated in time. NAGS deficiency is a congenital urea cycle disorder. Due to the lack of NAGS, patients often have high blood ammonia concentration, which may lead to acute death. As a rare disease, NAGS deficiency has few therapeutic drugs, and it is often difficult for patients to receive effective treatment. [0003] Carboglutamic acid, chemical name: N-carbamoyl-L-glutamic acid or (2S)-2-(carbamoylamino) glutaric acid, chemical formula: C 6 h 10 N 2 o 5 . This product is mainly used for the treatment of acute or chronic hyperammon...

Claims

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Application Information

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IPC IPC(8): C07C273/18C07C275/16
CPCC07C273/189C07C275/16
Inventor 阎智勇夏以顺张晓郭亚兵杨波
Owner WUHAN WUYAO SCI & TECH
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